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Water → Methyl 3-t-butyl-4-hydroxy-5-iodobenzoate

HRID 385030
ノート
印刷プレビュー

反応式

HRID 385030 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][C:14]=1[OH:15])[C:8]([O:10][CH3:11])=[O:9])([CH3:4])([CH3:3])[CH3:2].[I:16]N1C(=O)CCC1=O.FC(F)(F)S(O)(=O)=O.O>ClCCl.CO>[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([I:16])[C:14]=1[OH:15])[C:8]([O:10][CH3:11])=[O:9])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 62406Trifluoromethanesulfonic acidHCID 120273N-IodosuccinimideHCID 13207060Methyl 3-tert-butyl-4-hydroxybenzoate

生成物 1

HCID 12084815Methyl 3-t-butyl-4-hydroxy-5-iodobenzoate収率 94.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6344Dichloromethane溶媒

実験手順

Methyl 3-t-butyl-4-hydroxybenzoate (1.83 g) was dissolved in dichloromethane (24 mL) and methanol (3 mL), and N-iodosuccinimide (2.08 g) and trifluoromethanesulfonic acid (3 mL) were added to the solution, and then the mixture was stirred at room temperature for 15 minutes. Water was added to the reaction solution, and then the organic layer was separated. The organic layer was washed with 10% sodium thiosulfate and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (2.77 g) as a brown crystal.

後処理

  1. customthe organic layer was separated
  2. washThe organic layer was washed with 10% sodium thiosulfate and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-5c22d3a8a061459990ebdc6a40e1ca1c
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367843B2

反応ノート

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